CN103191689A - Production device of potassium dimethyldithiocarbamate and preparation method thereof - Google Patents
Production device of potassium dimethyldithiocarbamate and preparation method thereof Download PDFInfo
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- CN103191689A CN103191689A CN2013101484178A CN201310148417A CN103191689A CN 103191689 A CN103191689 A CN 103191689A CN 2013101484178 A CN2013101484178 A CN 2013101484178A CN 201310148417 A CN201310148417 A CN 201310148417A CN 103191689 A CN103191689 A CN 103191689A
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Abstract
The invention discloses a production device of potassium dimethyldithiocarbamate and a preparation method thereof. The production device comprises a reaction kettle, wherein a dimethylamine overhead tank, a sulfur dioxide overhead tank, a potassium hydroxide overhead tank and a soft water overhead tank are respectively communicated to the upper part of the reaction kettle through pipelines; and a filter and an end product storage tank are sequentially and respectively communicated with a reaction kettle discharging valve through pipelines. The production method comprises the steps of: respectively metering carbon disulfide, concentration potassium hydroxide solution with the concentration of 40%, concentration dimethylamine solution with the concentration of 50% and softened water in proportion by mass, firstly putting the concentration dimethylamine solution with the concentration of 50% into the reaction kettle, starting stirring, and introducing cooling media into a reaction kettle jacket and an inner cooling coil by utilizing a cooler; when the kettle temperature decreases to 5-20 DEG C, respectively adding the carbon disulfide and concentration potassium hydroxide solution with the concentration of 40% into the reaction kettle, then adding the softened water, after reacting for 100-150min, slowly opening the reaction kettle discharging valve, and sequentially pressing materials in the reaction kettle into a filter and the end product storage tank.
Description
Technical field
The present invention relates to process units and the production method of the U.S. potassium of a kind of liquid good fortune, belong to the chemical products production technical field.
Background technology
The U.S. potassium of good fortune (formal name used at school potassium dimethyldithiocarbamate) is light green, excitant ammonia flavor liquid is arranged that main application has: Industrial Wastewater Treatment; Heavy metal sinks lozenge; Paper industry; Disinfectant on chemical industry, daily-use chemical industry, coating and other industry; The polymerization inhibitor that the part high polymer is synthetic; Thiofide, butadiene-styrene rubber polymerization terminator etc.
In Treatment of Industrial Water, the excessive multiplication of bacterium algae can reduce heat transfer efficiency, makes equipment accelerate corrosion, perforation.Excessive bacterium algae can produce a large amount of foundry loam disabling facilities in the water of oil field, brings great hidden danger to production.In the industrial cooling circulating water system, adhering to of foundry loam and algae can reduce cooling tower and efficiency of heat exchanger, can cause pipeline blockage when serious, and direct economic loss is produced and brought in influence.Therefore, no matter domestic water still is water for industrial use and waste water, must control algae content in the various water bodys by artificial means, and adding the sterilization algae removal disinfectant is one of main means.Develop the low and residual littler preparation of environment of new germicidal efficiency height, toxicity and become focus new in the present industry.The U.S. potassium of good fortune is as disinfectant, and is easy to use, safety non-toxic, cheap, effect is remarkable, use a couple of days after, with regard to degradable, in the water treatment field large usage quantity.Before selecting the seedbed to grow seedlings, the container bag employing order method of growing seedlings, 1 ~ 2 of each container bag sowing, it is thick to broadcast back earthing 1.0 ~ 1.5cm, spraying mass concentration with watering can immediately is 3% the U.S. potassium dilution of good fortune, both soil is played disinfective action, and simultaneously soil and seed were connected airtight, be conducive to germination.This sterilization method is applied for many years.
At present, the U.S. potassium production of domestic good fortune mainly adopts dimethylamine, potassium hydroxide, carbon disulfide to react, and the U.S. process for synthesis of potassium of existing good fortune mainly contains following shortcoming:
1, owing to adopt atmospheric operation, carbon disulfide is easy to volatilize from reaction system, causes carbon disulfide unit consumption height, increases production cost on the one hand, on the one hand contaminated environment;
2, produce in two steps, earlier with (CH
3)
2NH and CS
2Reaction generates dimethyl dithiocarbamic acid, generates final products with the KOH reaction again, artificially prolongs the operating time;
3, poor stability, the domestic same industry firing accident once occurred and caused heavy economic losses.For this reason, develop a kind of carbon disulfide conversion ratio height, integrated cost is low, product yield is high, production operation safe ready, the U.S. potassium production method of good fortune with short production cycle, for industry development, improves the industry economic benefit, have important practical significance.
Summary of the invention
The technical problem to be solved in the present invention is in order to overcome the above-mentioned defective of the U.S. potassium production method of traditional good fortune, provide a kind of and improve feed stock conversion, reduce material loss that technological reason causes, reduce security risk, improve processing safety, shorten the process units of the U.S. potassium of liquid good fortune in product operation cycle.
In order to address the above problem, the present invention by the following technical solutions:
The process units of the U.S. potassium of a kind of liquid good fortune, comprise reactor, the top of described reactor is communicated with dimethylamine head tank, sulfur dioxide head tank, potassium hydroxide head tank and soft water head tank respectively by pipeline, the bottom of described reactor is connected with discharging valve of reaction kettle, and discharging valve of reaction kettle is communicated with filter and finished product basin successively by pipeline.
Below be the present invention to the further optimization of such scheme:
The outside of described reactor is provided with reacting kettle jacketing and interior cooling coil, described reacting kettle jacketing and interior cooling coil have cooler by pipeline connection, its objective is material in reactor is cooled off, the synergy that adds reacting kettle jacketing cooling, the cooling of reactor inner coil pipe is enough to take out reaction heat, shortens the reaction time;
Further optimize: on the connecting pipeline between discharging valve of reaction kettle and the filter circulating pump is installed, with circulating pump material is circulated.
Further optimize: the air compressor that is communicated with in parallel on the connecting pipeline between described dimethylamine head tank, sulfur dioxide head tank, potassium hydroxide head tank and soft water head tank and the reactor, the top of described reactor is equipped with atmospheric valve.
The present invention also provides the production method of the U.S. potassium of a kind of liquid good fortune, and this method may further comprise the steps:
1), carbon disulfide, concentration 40% potassium hydroxide solution, concentration 50% dimethylamine solution, demineralized water are entered corresponding sulfur dioxide head tank, potassium hydroxide head tank, dimethylamine head tank and soft water head tank separately respectively after according to quality proportioning 1:1.88-1.92:1.20-1.22:0.11-0.13 metering;
2), open the atmospheric valve of reactor upper end, earlier concentration is put into reactor from the dimethylamine head tank by the air pressure that air compressor provides for 50% dimethylamine solution, start stirring, feed cooling medium by cooler to reacting kettle jacketing and interior cooling coil;
When still temperature drop during to 5-20 ℃, carbon disulfide, 40% potassium hydroxide solution are added reactor from sulfur dioxide head tank, potassium hydroxide head tank by the air pressure that air compressor provides respectively, add demineralized water by the soft water head tank then, close atmospheric valve, the ON cycle pump;
3), pick up counting from the ON cycle pump, reacted 100-150 minute, the control temperature in the kettle is 15-35 ℃;
Reaction equation is as follows:
（CH
3）
2NH + CS
2 + KOH → (CH
3)
2NCS
2K + H
2O。
4), slowly open discharging valve of reaction kettle, enter the finished product basin after with circulating pump the reactor material being pressed into filter.
The present invention adopts such scheme, has the following advantages:
1, taking into full account dimethylamine and carbon disulfide reaction generation diformazan ammonia two bamic acids is these characteristics of exothermic reaction, adopt three groups of cooling mediums namely: reacting kettle jacketing, reactor inner coil pipe, outer circulation cooler take out the heat that reaction generates, reacting balance temperature drift can not occur and cause carbon disulfide loss and security incident.
2, except stirring, reactor self promotes the reaction, in the reactor bottom circulating pump is set, with pump material is circulated, strengthened the heat and mass of material, strengthened the mixing of materials degree, increased the mixing effect of material, bottoms material and reactor upper end material reaction situation is reached unanimity, reaction effect is good.
3, whole disposable adding reactors of material are easy and simple to handle slightly reacting under the pressure, constant product quality, and the quality index difference is little between each batch.
4, this technology makes the production cycle only for existing technology half, and single device production capacity doubles.
5, feed stock conversion improves, and the almost full entry reaction of dimethylamine and carbon disulfide does not almost have carbon disulfide in the finished product and dimethylamine is residual.
6, reaction mass correctly measures disposable adding reactor, the disposable quality requirement of producing that reaches of finished product need not be added the U.S. potassium concn of moisture adjusting good fortune again and reach quality index, and product directly enters the finished product basin, operate easylier, need not secondary and stir and to make material even.
The invention will be further described below in conjunction with drawings and Examples.
Description of drawings
Accompanying drawing 1 is the process chart that the U.S. potassium of liquid good fortune is produced in the embodiment of the invention.
Among the figure: 1-dimethylamine head tank; 2-sulfur dioxide head tank; 3-potassium hydroxide head tank; 4-soft water head tank; The 5-reactor; The 6-cooler; The 7-filter; 8-finished product basin; The 9-circulating pump; The 10-atmospheric valve; 11-reacting kettle jacketing and interior cooling coil; The 12-discharging valve of reaction kettle; The 13-air compressor.
The specific embodiment
Embodiment, as shown in Figure 1, the process units of the U.S. potassium of a kind of liquid good fortune, comprise reactor 5, the top of described reactor 5 is communicated with dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 respectively by pipeline, the bottom of described reactor 5 is connected with discharging valve of reaction kettle 12, and discharging valve of reaction kettle 12 is communicated with filter 7 and finished product basin 8 successively by pipeline.
The outside of described reactor 5 is provided with reacting kettle jacketing and interior cooling coil 11, described reacting kettle jacketing and interior cooling coil 11 have cooler 6 by pipeline connection, its objective is material in reactor is cooled off, the synergy that adds reacting kettle jacketing cooling, the cooling of reactor inner coil pipe is enough to take out reaction heat, shortens the reaction time;
On the connecting pipeline between discharging valve of reaction kettle 12 and the filter 7 circulating pump 9 is installed, with circulating pump 9 material is circulated.
The air compressor 13 that is communicated with in parallel on the connecting pipeline between described dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 and the reactor 5, the top of described reactor 5 is equipped with atmospheric valve 10.
The production method of the U.S. potassium of a kind of liquid good fortune may further comprise the steps:
1, accurately 540Kg concentration is that 50% dimethylamine solution, metering 450Kg carbon disulfide, 850Kg concentration are that 40% potassium hydroxide solution, 50Kg demineralized water enter corresponding dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 separately respectively;
2, open the atmospheric valve 10 of reactor 5 upper ends, earlier concentration is put into reactor 5 for the air pressure that 50% dimethylamine solution provides by air compressor 13 from dimethylamine head tank 1, start stirring, feed cooling mediums by cooler 6 to reacting kettle jacketing and interior cooling coil 11, when still temperature drop to 10 ℃, with carbon disulfide, 40% potassium hydroxide solution is respectively from sulfur dioxide head tank 2, potassium hydroxide head tank 3 adds reactor 5 by the air pressure that air compressor provides, add the 50Kg demineralized water by soft water head tank 4 then, close atmospheric valve 10, ON cycle pump 9;
3, pick up counting from ON cycle pump 9, reacted 120 minutes, the control temperature in the kettle is 15-30 ℃;
Reaction equation is as follows:
（CH
3）
2NH + CS
2 + KOH → (CH
3)
2NCS
2K + H
2O。
4, slowly open discharging valve of reaction kettle 12, enter finished product basin 8 after with circulating pump 9 the reactor material being pressed into filter 7.
Sample analysis finished product jar Nei Fumei potassium content is provided the quality analysis report.Single batch operation finishes.
The product quality indicator of preparation sees Table 1.
The U.S. potassium quality index of the good fortune of table 1 preparation
| Sequence number | Index name | Desired value | Analysis result |
| 1 | Outward appearance | Light yellow transparent liquid | Light yellow transparent liquid |
| 2 | Form and aspect, number≤ | 10 | 10 |
| 3 | Content (m/m), % 〉= | 50.0 | 50.46 |
| 4 | Free alkali, (in KOH, m/m) % | 0.05-0.50 | 0.12 |
| 5 | Density (D 4 20) , g/ml | 1.20-1.30 | 1.2646 |
| 6 | PH value | 9.5-12.5 | 10.8 |
Embodiment 2, as shown in Figure 1, the process units of the U.S. potassium of a kind of liquid good fortune, comprise reactor 5, the top of described reactor 5 is communicated with dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 respectively by pipeline, the bottom of described reactor 5 is connected with discharging valve of reaction kettle 12, and discharging valve of reaction kettle 12 is communicated with filter 7 and finished product basin 8 successively by pipeline.
The outside of described reactor 5 is provided with reacting kettle jacketing and interior cooling coil 11, described reacting kettle jacketing and interior cooling coil 11 have cooler 6 by pipeline connection, its objective is material in reactor is cooled off, the synergy that adds reacting kettle jacketing cooling, the cooling of reactor inner coil pipe is enough to take out reaction heat, shortens the reaction time;
On the connecting pipeline between discharging valve of reaction kettle 12 and the filter 7 circulating pump 9 is installed, with circulating pump 9 material is circulated.
Be communicated with air compressor 13 on the connecting pipeline between described dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 and the reactor 5, the top of described reactor 5 is equipped with atmospheric valve 10.
The U.S. potassium production method of a kind of liquid good fortune may further comprise the steps:
1, accurately measuring 578Kg concentration is that 50% dimethylamine solution, 478Kg carbon disulfide, 900Kg concentration are 40% potassium hydroxide solution and 55Kg demineralized water, enters corresponding dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 separately respectively;
2, open the atmospheric valve 10 of reactor 5 upper ends, earlier concentration is put into reactor 5 for the air pressure that 50% dimethylamine solution provides by air compressor from dimethylamine head tank 1, start stirring, feed cooling mediums by cooler 6 to reacting kettle jacketing and interior cooling coil 11, when still temperature drop to 15 ℃, with carbon disulfide, 40% potassium hydroxide solution is respectively from sulfur dioxide head tank 2, potassium hydroxide head tank 3 adds reactor 5 by the air pressure that air compressor provides, add the 55Kg demineralized water by soft water head tank 4 then, close atmospheric valve 10, ON cycle pump 9;
3, pick up counting from ON cycle pump 9, reacted 120 minutes, the control temperature in the kettle is 20-35 ℃;
Reaction equation is as follows:
（CH
3）
2NH + CS
2 + KOH → (CH
3)
2NCS
2K + H
2O。
4, slowly open discharging valve of reaction kettle 12, enter finished product basin 8 after with circulating pump 9 the reactor material being pressed into filter 7.
Sample analysis finished product jar Nei Fumei potassium content is provided the quality analysis report.Single batch operation finishes.
The product quality indicator of preparation sees Table 2.
The U.S. potassium quality index of the good fortune of table 2 preparation
| Sequence number | Index name | Desired value | Analysis result |
| 1 | Outward appearance | Light yellow transparent liquid | Light yellow transparent liquid |
| 2 | Form and aspect, number≤ | 10 | 10 |
| 3 | Content (m/m), % 〉= | 50.0 | 50.16 |
| 4 | Free alkali, (in KOH, m/m) % | 0.05-0.50 | 0.09 |
| 5 | Density (D 4 20) , g/ml | 1.20-1.30 | 1.2788 |
| 6 | PH value | 9.5-12.5 | 9.8 |
Embodiment 3, as shown in Figure 1, the process units of the U.S. potassium of a kind of liquid good fortune, comprise reactor 5, the top of described reactor 5 is communicated with dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 respectively by pipeline, the bottom of described reactor 5 is connected with discharging valve of reaction kettle 12, and discharging valve of reaction kettle 12 is communicated with filter 7 and finished product basin 8 successively by pipeline.
The outside of described reactor 5 is provided with reacting kettle jacketing and interior cooling coil 11, described reacting kettle jacketing and interior cooling coil 11 have cooler 6 by pipeline connection, its objective is material in reactor is cooled off, the synergy that adds reacting kettle jacketing cooling, the cooling of reactor inner coil pipe is enough to take out reaction heat, shortens the reaction time;
On the connecting pipeline between discharging valve of reaction kettle 12 and the filter 7 circulating pump 9 is installed, with circulating pump 9 material is circulated.
Be communicated with air compressor 13 on the connecting pipeline between described dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 and the reactor 5, the top of described reactor 5 is equipped with atmospheric valve 10.
The U.S. potassium production method of a kind of liquid good fortune may further comprise the steps:
1, accurately measuring 420Kg concentration is that 50% dimethylamine solution, 350Kg carbon disulfide, 660Kg concentration are 40% potassium hydroxide solution and 40Kg demineralized water, enters corresponding dimethylamine head tank 1, sulfur dioxide head tank 2, potassium hydroxide head tank 3 and soft water head tank 4 separately respectively;
2, open the atmospheric valve 10 of reactor 5 upper ends, earlier concentration is put into reactor 5 for the air pressure that 50% dimethylamine solution provides by air compressor from dimethylamine head tank 1, start stirring, feed cooling mediums by cooler 6 to reacting kettle jacketing and interior cooling coil 11, when still temperature drop to 10 ℃, with carbon disulfide, 40% potassium hydroxide solution is respectively from sulfur dioxide head tank 2, potassium hydroxide head tank 3 adds reactor 5 by the air pressure that air compressor provides, add the 40Kg demineralized water by soft water head tank 4 then, close atmospheric valve 10, ON cycle pump 9;
3, pick up counting from ON cycle pump 9, reacted 140 minutes, the control temperature in the kettle is 15-25 ℃;
Reaction equation is as follows:
（CH
3）
2NH + CS
2 + KOH → (CH
3)
2NCS
2K + H
2O。
4, slowly open discharging valve of reaction kettle 12, enter finished product basin 8 after with circulating pump 9 the reactor material being pressed into filter 7.
Sample analysis finished product jar Nei Fumei potassium content is provided the quality analysis report.Single batch operation finishes.
The product quality indicator of preparation sees Table 3.
The U.S. potassium quality index of the good fortune of table 3 preparation
| Sequence number | Index name | Desired value | Analysis result |
| 1 | Outward appearance | Light yellow transparent liquid | Light yellow transparent liquid |
| 2 | Form and aspect number≤ | 10 | 10 |
| 3 | Content (m/m) % 〉= | 50.0 | 50.62 |
| 4 | Free alkali, (in KOH, m/m) % | 0.05-0.50 | 0.24 |
| 5 | Density (D 4 20) g/ml | 1.20-1.30 | 1.2746 |
| 6 | PH value | 9.5-12.5 | 11.6 |
In above-described embodiment, the volume of described reactor is 1500L.
Claims (5)
1. the process units of the U.S. potassium of a liquid good fortune, comprise reactor (5), it is characterized in that: the top of described reactor (5) is communicated with dimethylamine head tank (1), sulfur dioxide head tank (2), potassium hydroxide head tank (3) and soft water head tank (4) respectively by pipeline, the bottom of described reactor (5) is connected with discharging valve of reaction kettle (12), and discharging valve of reaction kettle (12) is communicated with filter (7) and finished product basin (8) successively by pipeline.
2. the process units of the U.S. potassium of a kind of liquid good fortune according to claim 1, it is characterized in that: the outside of described reactor (5) is provided with reacting kettle jacketing and interior cooling coil (11), and described reacting kettle jacketing and interior cooling coil (11) have cooler (6) by pipeline connection.
3. the process units of the U.S. potassium of a kind of liquid good fortune according to claim 2 is characterized in that: described
On the connecting pipeline between discharging valve of reaction kettle (12) and the filter (7) circulating pump (9) is installed.
4. the process units of the U.S. potassium of a kind of liquid good fortune according to claim 3 is characterized in that:
The air compressor (13) that is communicated with in parallel on the connecting pipeline between described dimethylamine head tank (1), sulfur dioxide head tank (2), potassium hydroxide head tank (3) and soft water head tank (4) and the reactor (5), the top of described reactor (5) is equipped with atmospheric valve (10).
5. the production method of the U.S. potassium of liquid good fortune as claimed in claim 4, it is characterized in that: this method may further comprise the steps:
1), carbon disulfide, concentration 40% potassium hydroxide solution, concentration 50% dimethylamine solution, demineralized water are entered corresponding sulfur dioxide head tank, potassium hydroxide head tank, dimethylamine head tank and soft water head tank separately respectively after according to quality proportioning 1:1.88-1.92:1.20-1.22:0.11-0.13 metering;
2), open the atmospheric valve of reactor upper end, be earlier that 50% dimethylamine solution is put into reactor from the dimethylamine head tank with concentration, start stirring, by cooler to reacting kettle jacketing and in cooling coil feed cooling medium;
When still temperature drop during to 5-20 ℃, carbon disulfide, 40% potassium hydroxide solution are added reactor from sulfur dioxide head tank, potassium hydroxide head tank respectively, add demineralized water by the soft water head tank then, close atmospheric valve, the ON cycle pump;
3), pick up counting from the ON cycle pump, reacted 100-150 minute, the control temperature in the kettle is 15-35 ℃;
Reaction equation is as follows:
（CH
3）
2NH + CS
2 + KOH → (CH
3)
2NCS
2K + H
2O；
4), slowly open discharging valve of reaction kettle, enter the finished product basin after with circulating pump the reactor material being pressed into filter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265383A (en) * | 2018-10-08 | 2019-01-25 | 泰山医学院 | A kind of synthetic method of good fortune U.S. potassium and application in the treatment of waste water |
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| JPS6333358A (en) * | 1986-07-29 | 1988-02-13 | Idemitsu Petrochem Co Ltd | Production of dithiocarbamate |
| CN1299814A (en) * | 1999-12-16 | 2001-06-20 | 王继亭 | One-step preparation process of rubber sulfurizing promoter |
| US20040092704A1 (en) * | 2001-02-06 | 2004-05-13 | Graham Swift | Methods of synthesis of polysuccinimide, copolymers of polysuccinimide and derivatives thereof |
| CN101280537A (en) * | 2008-05-19 | 2008-10-08 | 贺明波 | Bleaching promotor and method for preparing the same |
| CN102516967A (en) * | 2011-12-02 | 2012-06-27 | 中国石油天然气集团公司 | Alkali/surfactant/polymer (ASP) flooding calcium-silicon-barium scale inhibitor and preparation method thereof |
| CN202478916U (en) * | 2012-02-03 | 2012-10-10 | 江苏泰格油墨有限公司 | Production device for liquid water-soluble resin |
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2013
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6333358A (en) * | 1986-07-29 | 1988-02-13 | Idemitsu Petrochem Co Ltd | Production of dithiocarbamate |
| CN1299814A (en) * | 1999-12-16 | 2001-06-20 | 王继亭 | One-step preparation process of rubber sulfurizing promoter |
| US20040092704A1 (en) * | 2001-02-06 | 2004-05-13 | Graham Swift | Methods of synthesis of polysuccinimide, copolymers of polysuccinimide and derivatives thereof |
| CN101280537A (en) * | 2008-05-19 | 2008-10-08 | 贺明波 | Bleaching promotor and method for preparing the same |
| CN102516967A (en) * | 2011-12-02 | 2012-06-27 | 中国石油天然气集团公司 | Alkali/surfactant/polymer (ASP) flooding calcium-silicon-barium scale inhibitor and preparation method thereof |
| CN202478916U (en) * | 2012-02-03 | 2012-10-10 | 江苏泰格油墨有限公司 | Production device for liquid water-soluble resin |
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| CN109265383A (en) * | 2018-10-08 | 2019-01-25 | 泰山医学院 | A kind of synthetic method of good fortune U.S. potassium and application in the treatment of waste water |
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